Index: Exp. No. Name of Experiment Page No. Date Grade Signature of Faculty

INDEX
Exp. Signature
Name of Experiment Page No. Date Grade
No. of Faculty
To prepare Aspirin from Acetic
anhydride and salicylic acid and to
1 02--05
determine its percentage yield and
melting point.
To prepare P-acetyl aminophenol
2 and to determine its percentage 06--08
yield.
To prepare Anthraquinone from
3 anthracene, acetic acid and to 09--11
determine its percentage yield.
To prepare Acetanilide from aniline,
4 acetic anhydride, acetic acid and to 12--14
To prepare methyl salicylate by
5 esterification of salicylic acid and to 15--17
To extract sugar from given sample
6 18--19
of beet.
To prepare Nitrobenzene by method
7 20--22
of direct nitration.
To prepare phenolphthalein form
8 phenol and Pthalic anhydride and to 23--25
To prepare Prussian blue dye from 26--28
potassium ferro cynaide and ferrous
9
sulfate and to determine its practical
yield.
To prepare Acetaminophen from p- 29--32
aminophenol, acetic anhydride and
10
to determine its percentage yield
and melting point.
Chemical Process Industries II Lab Manual
By: - Prof. D. N. Yadav

Government Engineering College Valsad
Chemical Process Industries-II
Lab Manual
Experiment No.1 Preparation of Aspirin Date:- ___/___/2018
Aim: To prepare Aspirin from Acetic anhydride and salicylic acid and to determine its
percentage yield and melting point.
Apparatus: Beaker (3Nos.), glass rods for mixing, measuring cylinder, pipette, conical flasks,
heating mantle, filtration assembly, Ice Bath.
Chemicals: Salicylic Acid, Acetic Anhydride, Sulfuric Acid, Water, Ethanol.
Reaction
Procedure
 Weigh accurately 10gm of salicylic acid, heat it over hot plate to remove moisture and
place it in a watch glass.
 Measure accurately 15ml of acetic anhydride and pour it into a conical flask.
 Add both the pre weighed salicylic acid and acetic anhydride in a round bottom flask.
 To this mixture, slowly add 5 drops of concentrated sulfuric acid.
 Gently heat the flask in a boiling water bath at 60-70°C for about 10 minutes.
 Because the reaction is slightly exothermic, a small temperature rise can be detected.
 Remove the flask from the hot water bath and add 10 mL of deionized ice water to
decompose any excess acetic anhydride. Chill the solution in an ice bath until crystals of
aspirin no longer form, stirring occasionally to decompose residual acetic anhydride. If
oil" appears instead of a solid, reheat the flask in the hot water bath until the oil
disappears and again cool.
 Add 15 mL of cold water to the flask, swirl, and chill again. Pour the liquid and the
crystals of aspirin onto the filter paper.
 Repeat until the transfer of the crystals to the filter paper is complete.
 Determine the mass of the crude aspirin crystals.
Purification of Aspirin
 The major impurity in aspirin is salicylic acid. It can be removed by a recrystallization.
 Place the aspirin crystals in a 100-mL beaker. Add 8 mL of ethanol and 25 mL of water.
Page 2 of 32
Lab Manual
 Warm the mixture in a 60°C water bath (no flame, use a hot plate or a hot water bath).
Warm the mixture until the aspirin dissolves.
 Cover the beaker with a watch glass, remove it from the heat, and set it aside to cool
slowly. Set the beaker in an ice bath. Beautiful needle-like crystals of acetylsalicylic acid
form.
 Collect the aspirin by filtration. Wash the crystals with two 10-mL volumes of ice water.
If time does not permit, place the filter paper and aspirin sample on a watch glass and
allow them to air-dry.
 Transfer the dry aspirin crystals to a pre-weighed sample container.
 Determine the mass of the aspirin crystals.
Determination of Melting Point of the Aspirin Sample

 Fill a capillary melting point tube to a depth of 0.2 cm with the recrystallized aspirin.
 Place the capillary tube in the melting point apparatus. Determine its melting point.
 Pure aspirin melts at 135°C.
 The aspirin sample should be labeled with your name, the mass of the aspirin, the
percent yield, and its melting point.
Page 3 of 32
Lab Manual
Observations
 Amount of salicylic acid taken : ______ gm
 Amount of acetic anhydride taken : ______ ml
 Amount of sulfuric acid added : ______ drops
Calculations:
Theoretical Yield
The mole ratios are 1:1:1 so one mole salicylic acid reacts with one mole acetic anhydride to
produce one mole of aspirin.
Molar mass of salicylic acid = 138.1 gm/mole
Molar mass of acetic anhydride = 102 gm/mole; 1.082gm/ml density
Molar mass of aspirin = 180.2 gm/mole
Moles of salicylic acid = mass of salicylic acid taken /molar mass
= gm/ 138.1
= moles salicylic acid
Grams of acetic anhydride = Volume * Density
= ml acetic anhydride x 1.082 gm/ml
= gm
Moles of acetic anhydride = mass of acetic anhydride taken /molar mass
= gm/102
= moles
Therefore the limiting reactant is salicylic acid and acetic anhydride is in excess.
The most aspirin that can be made under these conditions is ________ moles.
Finding the Theoretical Yield,
Theoretical Yield = moles of aspirin x molar mass of aspirin
= moles x gm/mole
= gms
Hence, 138 gm of salicylic acid gives 180gm of Aspirin

→ 10 gm of salicylic acid gives ?
Grams of Aspirin obtained = _____X_____
= gm
Practical Yield
Weight of aspirin obtained on drying : _______ gm
Page 4 of 32
Lab Manual
% yield of Aspirin
% yield = Practical Yield X 100
Theoretical Yield
= ________
Melting point
Melting point of aspirin as obtained : ______ °C
Results:
 Theoretical yield of Aspirin : ______
 Experimental yield of Aspirin : ______
 % yield of Aspirin prepared : ______
 Melting point of Aspirin prepared : ______
- - - -
***
Page 5 of 32
Lab Manual
Experiment No.2 Preparation of P-Acetyl aminophenol Date: - ___/___/2018
Aim: To prepare P- Acetyl aminophenol.
Apparatus: Glass Beakers, Conical Flask, Stirrer, Thermometer, Filtration Assembly, Weighing
Scale, Heating Mantle, Burette, Pipette.
Chemicals: p-amino phenol, water, acetic anhydride
Reaction:
Procedure :
 Precisely measure out 5.5gm of p-amino phenol and suspend it in 15ml of water
contained in 100ml beaker or a conical flask.
 Also measure out 6ml of acetic anhydride in a measuring cylinder.
 To the pre weighed p-amino phenol adds 6ml of acetic anhydride.
 Stir and warm the mixture in order to dissolve the solids.
 After 10minutes of heating cool the solution to room temperature and later add 10ml of
chilled water.
 P- Acetyl aminophenol crystals shall be formed, filter out the same.
 Wash the obtained filters with cold water.
 Dry the crystals and measure the final weight obtained.
Page 6 of 32
Lab Manual
Observations
 Amount of p-aminophenol taken : ______ gm
 Amount of water added : ______ ml
Calculations:
Theoretical Yield
Molar mass of p-aminophenol =109.1g/mol
Molar mass of acetic anhydride = 102.1 g/mol
Moles of p-aminophenol = mass of p-aminophenol taken /molar mass

= g/ (109.1g/mol)
= mol
Moles of acetic anhydride = mass of acetic anhydride taken/molar mass

= g/ (102.1g/mol)
= mol
Hence, Theoretical Yield

109 gm of p-aminophenol gives 177 gm of P- Acetyl aminophenol
→ 5.5 gm of salicylic acid gives ? gm of P- Acetyl aminophenol
Grams of Acetaminophen obtained = _____X_____
= gm
Practical Yield
Weight of P-Ethoxyacetanilide obtained on drying : _______ gm
Page 7 of 32
Lab Manual
% yield of P-Ethoxyacetanilide
Theoretical Yield
= ________
Results:
 Theoretical yield of P-Ethoxyacetanilide : ______ gm
 Experimental yield of P-Ethoxyacetanilide : ______ gm
 % yield of P-Ethoxyacetanilide prepared : ______
 Melting point of P-Ethoxyacetanilide prepared : ______
- - - -
***
Page 8 of 32
Lab Manual
Experiment No.3 Preparation of Anthraquinone Date: - ___/___/2018
Aim: To prepare Anthraquinone from anthracene, nitric acid and to determine its
percentage yield.
Chemicals: Anthracene, Water, Chromium Trioxide, Glacial Acetic Acid.
Reaction:
Procedure:
 Take about 1gm of Anthracene in a dry beaker.
 Take about 10ml of glacial acetic acid in a measuring cylinder.
 Transfer the pre weighted anthracene and glacial acetic acid in a round bottom flask
fitted with a reflux condenser.
 Separately take 2gm of Chromium trioxide and dissolve it in 2ml of water and 5ml of
glacial acetic acid. Transfer the prepared solution to a burette.
 Heat the system slowly for 10min until the acetic acid boils and greater part of
anthracene goes into the solution mixture.
 After 10mins of heating slowly drop wise add the solution of chromium trioxide and
acetic acid through the centre of the reflux condenser. The flow rate should be such that
the addition takes about 10min of time.
 After the addition of Chromium Trioxide solution is complete, continue boiling for
another 10minutes, and allow the solution to cool to room temperature.
 Later dissolve the crystals formed by adding 10ml of chilled water and filter out the
crystals.
 Crude anthracene separates as greenish grey powder.
Determination of Melting Point of the Anthraquinone Sample

 Fill a capillary melting point tube to a depth of 0.2 cm with the recrystallized
Anthraquinone.
 The melting point of Anthraquinone is 286°C.
 The Anthraquinone sample should be labeled with your name, the mass of the
acetaminophen, the percent yield, and its melting point.
Page 9 of 32
Lab Manual
Observations
 Amount of Anthracene taken : ______ gm
 Amount of Acetic Acid taken : ______ ml
 Amount of Chromium Trioxide soln. taken : ______ ml
Calculations:
Theoretical Yield
Molar mass of anthracene = 178.23 g/mol
Molar mass of acetic acid = 63.01 g/mol
Molar mass of Anthraquinone = 208 g/mol
Moles of anthracene = mass of anthracene taken/molar mass
= g/ (178.23 g/mol)
= mol
Grams of acetic acid taken = Volume * Density
= ml acetic acid taken x 1.05 gm/ml
= gm
Moles of acetic acid taken = mass of acetic acid taken / molar mass
= g/ (60.05 g/mol)
= mol
Theoretical Yield
Hence, 178.23 gm of Anthracene gives 208 gm of Anthraquinone
→ 01 gm of Anthracene gives ? gm of Anthraquinone
Grams of Anthraquinone obtained = _____X_____
= gm
Practical Yield
Weight of Anthraquinone obtained on drying : _______ gm
Page 10 of 32
Lab Manual
% yield of Anthraquinone
Theoretical Yield
= ________
Melting point
Melting point of Anthraquinone as obtained : ______ °C
Results:
 Theoretical yield of Anthraquinone : ______ gm
 Experimental yield of Anthraquinone : ______ gm
 % yield of Anthraquinone prepared : ______
 Melting point of Anthraquinone prepared : ______
- - - -
***
Page 11 of 32
Lab Manual
Experiment No.4 Preparation of Acetanilide Date: - ___/___/2018
Aim: To prepare Acetanilide from aniline, acetic anhydride, acetic acid and to
Apparatus: Beaker (3Nos.), Round bottom flask, glass rods for mixing, measuring cylinder,
pipette, conical flasks, heating mantle, filtration assembly, Ice Bath.
Chemicals: Aniline, Acetic Anhydride, Charcoal & Water.
Reaction:
Procedure:
 Firstly measure the empty beaker/conical flask to its smallest gms in which the reaction
shall take place.
 Take exactly 10ml of aniline, 10ml of acetic acid, 10ml of acetic anhydride in a three
different measuring cylinders.
 Mix all the three chemicals stepwise into a beaker and boil it for 30mins.
 Pour the heated mixture in a beaker containing 200ml cold water with constant stirring
with glass rod.
 Acetanilide crystals will be formed.
 To the crystal formed add 1ml of activated charcoal and boil it in 150ml distilled water.
The color impurities formed shall be removed by filtering the mixture after allowing it to
cool.
 Set the crystals formed to cool in an ice chilled bath.
 Filter out the crystals obtained, dry them and measure their weight.
Determination of Melting Point of the Acetanilide Sample

 Fill a capillary melting point tube to a depth of 0.2 cm with the recrystallized Acetanilide.
 The melting point of Acetanilide is 114.3C.
 The Acetanilide sample should be labeled with your name, the mass of the
Page 12 of 32
Lab Manual
Observations
 Amount of Aniline taken : ______ ml
 Amount of acetic acid taken : ______ ml
 Charcoal used : ______ gm
Calculations:
Theoretical Yield
Molar mass of aniline = 93.13 g/mol
Molar mass of acetic acid = 60.05 g/mol
Molar mass of acetanilide = 135.17 g/mol
Grams of aniline taken = Volume * Density
= ml aniline taken x 1.0217 gm/ml
= gm
Moles of aniline = mass of aniline / molar mass

= g/ (93.13 g/mol)
= mol
Grams of acetic anhydride taken = Volume * Density

= ml acetic anhydride taken x 1.08 gm/ml
= gm
Moles of acetic anhydride taken = mass of acetic anhydride/ molar mass

= g/ (102.09 g/mol)
= mol
Grams of acetic acid taken = Volume * Density

= ml acetic acid taken x 1.05 gm/ml
= gm
Moles of acetic acid taken = mass of acetic acid taken / molar mass
= g/ (60.05 g/mol)
= mol
Since there are more moles of aniline is than that of acetic anhydride, acetic anhydride is used
up first as the reaction proceeds. We can conclude that Aniline is in excess and Acetic
Anhydride is the limiting reagent.

Page 13 of 32
Lab Manual

Theoretical Yield = moles of acetanilide x molar mass of acetanilide
= mol x g/mol
= g
Hence, 102 gm of acetic anhydride gives 135 gm of Acetanilide

→ gm of acetic anhydride gives ? gm of Acetanilide
Grams of Acetanilide obtained = _____X_____
= gm
Practical Yield
Weight of Acetanilide obtained on drying : _______ gm
% yield of Acetanilide
Theoretical Yield
= ________
Melting point
Melting point of Acetanilide as obtained : ______ °C
Results:
 Theoretical yield of Acetanilide : ______ gm
 Experimental yield of Acetanilide : ______ gm
 % yield of Acetanilide prepared : ______
 Melting point of Acetanilide prepared : ______
- - - -
***
Page 14 of 32
Lab Manual
Experiment No.5 Preparation of Methyl Salicylate Date: - ___/___/2018
Aim: To prepare methyl salicylate by esterification of salicylic acid and to determine

its percentage yield.
Apparatus: Burner, Beaker , Round bottom flask, Glass rods for mixing, Measuring cylinder,
pipette, conical flasks, heating mantle, Filtration assembly, Ice Bath.
Chemicals: Salicylic Acid, Water, Methanol, conc. H2SO4.
Reaction:
Procedure:
 Firstly weigh accurately 14gm salicylic acid in a watch glass.
 Also measure out 40ml absolute methanol and 5 drops conc. Sulphuric acid.
 Place the previously weighed 14gm salicylic acid in a Round bottom flask and to this add
40ml absolute methanol and add 5 drops of conc. Sulphuric acid. Continue stirring while
adding the reactants in the round bottom flask with glass rods.
 Fit with reflux condenser and reflux by heating on water bath for 5 hours.
 Distill off the excess methanol and allow it to cool.
 Pour the residue in about 125ml water in a separating funnel.
 Shake and allow it cool.
 Separate in two layers, cool lower milky white layer and wash with sodium bicarbonate
solution and water.
 Dry over 5grams of anhydrous magnesium sulfate for at least 30min.
 If emulsion is formed during washing add 10ml CCl4.s
Page 15 of 32
Lab Manual
Observations
 Amount of Salicylic Acid taken : ______ ml
 Amount of conc. H2SO4 taken : ______ ml
 Amount of Methanol taken : ______ ml
 CCl4 used : ______ gm
Calculations:
Theoretical Yield
Molar mass of Salicylic Acid = 138.121 g/mol
Molar mass of Methanol = 32.04 g/mol
Molar mass of Sulfuric Acid = 98.079 g/mol
Grams of Methanol taken = Volume * Density

= ml Methanol taken x 0.7918 gm/ml
= gm
Moles of Methanol = mass of Methanol / molar mass

= g/ (32.04 g/mol)
= mol
Grams of Salicylic Acid taken = gm
Since there are more grams of methanol than that of salicylic acid, salicylic acid is used up first
as the reaction proceeds. We can conclude that Methanol is in excess and Salicylic Acid is the
limiting reagent.

Theoretical Yield
Hence, 138 gm of salicylic acid gives 152 gm of Methyl Salicylate

→ 14 gm of salicylic acid gives ? gm of Methyl Salicylate
Grams of Methyl Salicylate obtained = _____X_____
= gm
Page 16 of 32
Lab Manual
Practical Yield
Weight of Methyl Salicylate obtained on drying : _______ gm
% yield of Methyl Salicylate

Theoretical Yield
= ________
Results:
 Theoretical yield of Methyl Salicylate : ______ gm
 Experimental yield of Methyl Salicylate : ______ gm
 % yield of Methyl Salicylate prepared : ______
- - - -
***
Page 17 of 32
Lab Manual
Experiment No.6 Extraction of Sugar from Beet Date: - ___/___/2018
Aim: To extract sugar from beet.

Apparatus: Burner, Evaporating dish, beaker, slicers, tripod, wire mesh, weighing scale.
Chemicals: Sugar Beet, Water, Dry Ice, Ethanol.
Procedure : (1)
 Take a fresh beet and wash thoroughly with water.
 Cut down the beet into several long and thin slices. These are known as Cassettes.
 Measure accurately 35gm of beat cassettes.
 Fill the round bottom flask with 100ml water (preferably enough that all beet must be
submerged in the water) and add the pre weighed beat cassettes to it.
 Heat the flask for at least 30min and later filter the hot sugar solution.
 Add approximately 0.2gm of CaO to the filtered solution and boil it for 5min.
 After boiling filter out the solution and add 2pieces of dry ice and boil until its volume is
approximately 1ml.
 Prepare a 10-30ml ethanol and transfer it to the solution with continuous stirring. Allow
the sugar to harden.
 Repeat this procedure until all bounded sugar is crystallized.
 Filter the obtained sugar, dry them and weigh it.
Procedure : (2)
 Take a fresh beet and wash thoroughly with water.
 Cut down the beet into several long and thin slices. These are known as Cassettes.
 Measure accurately 35gm of beat cassettes.
 Fill the round bottom flask with 100ml water (preferably enough that all beet must be
submerged in the water) and add the pre weighed beat cassettes to it.
 Heat the flask for at least 30min.
 Meanwhile take an evaporating dish and measure its weight correctly up to two decimal
places.
 Transfer the liquid from the round bottom flask (after been heated for 30min) to the
evaporating dish and start heating to evaporate water.
 Leave the solution to cool and check for sugar crystals.
 Add more beet extract to the evaporating dish and repeat the above steps.
 Once all of the beet extract has been evaporated weigh out the evaporating dish and
from which you can determine the practical amount of sugar formed.
Page 18 of 32
Lab Manual
Observations
 Whole Mass of Sugar beet taken : ______ ml
 Mass of Sugar Beet taken : ______ ml
 Amount of Ethanol taken : ______ ml
 Amount of CaO added : ______ gm
 Weight of Empty Evaporating dish : ______ gm
Calculations:
Amount of Sugar Obtained = (Wt. of evaporating dish with Sugar Crystals) ( wt. of empty
evaporating dish)
% Yield of Sugar Obtained = Weight of sugar extracted

Weight of Sugar beet taken
Results:
 Experimental yield of Sugar Produced : ______ gm
 % yield of Sugar Produced : ______
- - - -
***
Page 19 of 32
Lab Manual
Experiment No.7 Preparation of Nitrobenzene Date: - ___/___/2018
Aim: To prepare Nitrobenzene by direct nitration of benzene.

Apparatus: Round bottom flask, Beakers, Conical Flask, Condenser, Weighing Scale,
Measuring Cylinders, Heating Mantle, Water Bath, Thermometer.
Chemicals: Nitric Acid, Sulfuric Acid, Benzene
Reaction:
Procedure :
 Precisely measure out 35ml of Nitric Acid, 40ml conc. Sulfuric Acid.
 As the preparation of nitrobenzene is an exothermic reaction heat is evolved, hence to
keep a check on temperature immerse the round bottom flask in which chemicals are to
be mixed and reacted in a chilled water bath.
 Place 35ml of nitric acid to the 500ml round bottom flask kept in water bath and add
40ml conc. Sulfuric Acid slowly to the same. Measure the temperature with the help of
thermometer and slowly add 29ml of benzene.
 The benzene should be added 3ml at a time and the content of the flask should be
mixed thoroughly after each addition, special care should be taken that the
temperature of the system should not be allowed to rise above 50°C. If necessary
submerge the round bottom flask into a new chilled water bath.
 Once all the benzene is added fit a reflux water condenser to the round bottom flask
and place the later in water bath maintained at 60°C for 1hr 30min. During this period
the flask should be withdrawn from time to time and must be vigorously shaken in order
to break up nitrobenzene layer which would otherwise float on dense acid layer below.
 After 45min of heating pour the contents of flask into large excess of cold water
(approx. 300ml) in which nitrobenzene being heavier than water sinks to bottom. Stir
the mixture vigorously in order to wash out as much as acid as possible from the
nitrobenzene. Decant of as much as possible of aqueous layer from the solution and
later transfer it to separating funnel.
 Shake it vigorously with equal volume of cold water. Allow nitrobenzene to separate
again and run it off.
 Repeat the washing using dil. Na2CO3 solution. Na2CO3 solution should be added until
there is no evolution of CO2 gas.
 Nitrobenzene is thus separated. Transfer the Nitrobenzene to a small conical flask and
small granual CaCl2. Shake the mixture until it is clear liquid.
Page 20 of 32
Lab Manual
Observations
 Volume of nitric acid taken : ______ ml
 Volume of sulfuric acid taken : ______ ml
 Volume of benzene taken : ______ ml
 Volume of coldwater taken : ______ ml
 Density of Nitrobenzene : 1.20 g/ml
Theoretical Yield
Molar mass of Nitric Acid = 63.01 g/mol
Molar mass of Benzene = 78.11 g/mol
Grams of Nitric Acid taken = Volume * Density

= ml Nitric Acid taken x 1.42 gm/ml
= gm
Moles of Nitric Acid = mass of Nitric Acid / molar mass

= g/ (63.01g/mol)
= mol
Grams of Sulfuric Acid taken = Volume * Density

= ml Sulfuric Acid taken x 1.83 gm/ml
= gm
Moles of Sulfuric Acid = mass of Sulfuric Acid / molar mass

= g/ (98.079 g/mol)
= mol
Grams of Benzene taken = Volume * Density

= ml Benzene taken x 0.8767 gm/ml
= gm
Moles of Benzene = mass of Benzene / molar mass

= g/ (78.11 g/mol)
= mol
Since there are more grams of Nitric Acid and Sulfuric Acid than that of Benzene, Benzene is
used up first as the reaction proceeds. We can conclude that Nitric Acid and Sulfuric Acid are
in excess and Benzene is the limiting reagent.
Page 21 of 32
Lab Manual

Theoretical Yield
Hence, 78 gm of benzene gives 123 gm of Nitrobenzene

→ 25.42 gm of benzene gives ? gm of Nitrobenzene
Grams of Nitrobenzene obtained = _____X_____
= gm
Practical Yield
Volume of Nitrobenzene Obtained : _______ ml
Grams of Nitrobenzene obtained = Volume * Density

= ml Nitrobenzene obtained x gm/ml
= gm
% yield of Nitrobenzene
Theoretical Yield
= ________
Results:
 Theoretical yield of Nitrobenzene : ______ gm
 Experimental yield of Nitrobenzene : ______ gm
 % yield of Nitrobenzene prepared : ______
- - - -
***
Page 22 of 32
Lab Manual
Experiment No.8 Preparation of Phenolphthalein Date: - ___/___/2018
Aim: To prepare phenolphthalein form phenol and phatlic anhydride and to

Apparatus: Glass Beakers, Conical Flask, Stirrer, Thermometer, Filtration Assembly, Weighing
Scale, Heating Mantle, Burette, Pipette .
Chemicals: Phenol , Pthalic anhydride crystals, conc. H 2SO4, conc. NaOH Soln., Absolute
Alcohol
Reaction:
Procedure :
 Precisely measure out 18.8 gm of Phenol and 14.5 gm of Pthalic anhydride and 8ml of
conc. sulphuric acid.
 Firstly add the phenol into a round bottom flask, secondly add Pthalic anhydride to the
same and later add the sulphuric acid slowly to the mixture.
 Heat the mixture in an oil bath at 120°C for about 4 hours.
 After the heating the reddish oily product is poured into excess amount of cold water
(preferably 500ml).
 Excess phenol is removed by steam distillation.
 The residual product is filtered and washed with water.
 It is dissolved in aqueous sodium hydroxide solution (10%) and the clear solution is
acidified with acetic acid and few drops of hydrochloric acid.
 Allow the mixture to stand overnight, the separated product is filtered, dried and
weighed.
 The crude product is purified by refluxing with excess alcohol (5ml of absolute alcohol
for each gram of product obtained) and decolorized by charcoal.
Page 23 of 32
Lab Manual
Observations
 Volume of phenol taken : ______ ml/gm
 Weight of Pthalic anhydride taken : ______ gm
 Volume of sulfuric acid taken : ______ ml
 Volume of ethanol added : ______ ml
 Volume of coldwater taken : ______ ml
Theoretical Yield
Molar mass of Phenol = 94.1124 g/mol
Molar mass of Pthalic Anhydride = 148.1 g/mol
Grams of Phenol taken = Volume * Density

= ml Phenol taken x 1.07 gm/ml
= gm
Moles of Phenol = mass of Nitric Acid / molar mass

= g/ (63.01g/mol)
= mol
Grams of Sulfuric Acid taken = Volume * Density

= ml Sulfuric Acid taken x 1.83 gm/ml
= gm
Moles of Sulfuric Acid = mass of Sulfuric Acid / molar mass

= g/ (98.079 g/mol)
= mol
Since there are more grams of Phenol than that of Pthalic anhydride, Phenol is used up first as
the reaction proceeds. We can conclude that Phenol is in excess and Pthalic anhydride is the
limiting reagent.
Page 24 of 32
Lab Manual
Theoretical Yield
Hence, 148 gm of Pthalic anhydride gives 123 gm of Phenolphthalein

→ gm of Pthalic anhydride gives ? gm of Phenolphthalein
Grams of Phenolphthalein obtained = _____X_____
=________ gm
Practical Yield
Grams of Phenolphthalein obtained =________ gm
% yield of Phenolphthalein
Theoretical Yield
= ________
Results:
 Theoretical yield of Phenolphthalein : ______ gm
 Experimental yield of Phenolphthalein : ______ gm
 % yield of Phenolphthalein prepared : ______
- - - -
***
Page 25 of 32
Lab Manual
Experiment No.9 Preparation of Prussian Blue Date: - ___/___/2018
Aim: To prepare Prussian blue from Potassium Ferro Cyanide and Ferrous Ammonium
Sulfate.
Apparatus: Beaker, glass rods for mixing, measuring cylinder, pipette, conical flasks, heating
mantle, filtration assembly, Ice Bath.
Chemicals: Potassium Ferro Cyanide ,Ferric Chloride, water.
Reaction:
4FeCl36H2O + 3K4(Fe(CN)6)3H2O  Fe4(Fe(CN)6)314H2O +12 KCl
Procedure:
 Precisely measure out 4gm of ferric chloride and transfer it to 100ml beaker containing
5ml distilled water and measure 2gm of potassium ferrocynaide in 5ml of water
contained in another 100ml beaker.
 Prepare Prussian Blue dye by transferring the potassium ferrocynaide solution into color
ferric chloride solution with constant stirring.
 Blue color crystals are precipitated from the solution.
 Filter out the crystals, dry them and determine its practical yield.
Page 26 of 32
Lab Manual
Observations
 Amount of Potassium Cyanide taken : ______ gm
 Amount of Ferrous Ammonium Sulfate taken : ______ gm
Calculations:
Theoretical Yield
Molar mass of Potassium Ferro Cyanide = g/mol
Molar mass of Ferrous Ammonium Sulfate = g/mol
Moles of Potassium Cyanide = mass of Potassium Ferro Cyanide taken /molar

mass
= g/ (368.35 g/mol)
= mol
Moles of Ferrous Ammonium Sulfate = mass of Ferrous Ammonium Sulfate taken/molar

mass
= g/ (284.05 g/mol)
= mol
Hence, Theoretical Yield

347 gm of Potassium Ferro Cyanide gives 860 gm of Prussian Blue
→ 4.0 gm of Potassium Ferro Cyanide gives ? gm of Prussian Blue
Grams of Prussian Blue obtained = _____X_____
= gm
Practical Yield
Weight of Prussian blue obtained on drying : _______ gm
Page 27 of 32
Lab Manual
% yield of Prussian Blue

Theoretical Yield
= ________
Results:
 Theoretical yield of Prussian Blue : ______ gm
 Experimental yield of Prussian Blue : ______ gm
 % yield of Prussian Blue prepared : ______
- - - -
***
Page 28 of 32
Lab Manual
Experiment No.10 Preparation of Acetaminophen Date: - ___/___/2018
Aim: To prepare Acetaminophen from p-aminophenol, acetic anhydride and to

determine its percentage yield and melting point.
Chemicals: P-amino phenol, Acetic anhydride, Phosphoric Acid.
Reaction:
Procedure:
 Fill a 400-mL beaker about half full with water. Place the beaker and water on a hot
plate and bring to a boil.
 Weigh out 1.5 g of p-aminophenol and transfer it into a 125-mL Erlenmeyer flask. Add
25 mL of water. Add 20 drops of concentrated phosphoric acid, H 3PO4, and swirl the
flask until all of the amine dissolves. If not, add a few more drops of phosphoric acid.
 Turn off the hot plate. Place the flask in the hot water. Carefully add 2 mL of acetic
anhydride to the flask. Leave the flask in the warm water for 10 minutes.
 Remove the flask and place it an ice-water bath. Stir the mixture to crystallize the
acetaminophen. You may need to scratch the walls of the flask to start the
crystallization. If no crystals appear, add a small seed of acetaminophen to start the
crystal formation. Allow the flask to stay in the ice-water bath for 30 minutes.
 Collect the crystals in a Buchner funnel using vacuum filtration.
 Wash the crystals with 10 mL of cold water. Allow the crystals to dry.
 Determine the mass of the crude acetaminophen.
Purification of Acetaminophen
 Place the crude acetaminophen in a 100-mL beaker. Add 20 mL of water and heat on a
hot plate until the crystals dissolve. If the solution boils and crystals remain, add another
10 mL of water.
Page 29 of 32
Lab Manual
 Remove the beaker and allow the solution to cool. When crystals begin to appear, place
the beaker in an ice bath for 20 minutes. If no crystals appear, scratch the inside walls of
the beaker.
 Collect the crystals using the Buchner filtration apparatus. Wash with 10 mL of cold
water.
 Transfer the filter paper and crystals to a watch glass and let dry.
 Determine the mass of the purified acetaminophen.
Determination of Melting Point of the Acetaminophen Sample

 Fill a capillary melting point tube to a depth of 0.2 cm with the recrystallized
acetaminophen.
 The melting point of acetaminophen is 169-171°C. p-aminophenol melts at 189-190°C.
 The acetaminophen sample should be labeled with your name, the mass of the
Page 30 of 32
Lab Manual
Observations
 Amount of p-aminophenol taken : ______ gm
 Amount of phosphoric acid added : ______ drops
Calculations:
Theoretical Yield
Molar mass of p-aminophenol =109.1g/mol
Molar mass of Acetaminophen =151.169 g/mol
Moles of p-aminophenol = mass of p-aminophenol taken /molar mass
= g/ (109.1g/mol)
= mol
Moles of acetic anhydride = mass of acetic anhydride taken/molar mass
= g/ (102.1g/mol)
= mol
From the balanced chemical equation we know that for every mole of p-aminophenol and
acetic acid one mole of acetaminophen is produced.
Since there are more moles of acetic anhydride than p-aminophenol, p-aminophenol is used up
first as the reaction proceeds. We can conclude that acetic anhydride is in excess and p-
aminophenol is the limiting reagent.
Therefore, no. moles of p-aminophenol = no. of acetaminophen produced

Theoretical Yield = moles of acetaminophen that can be produced x molar mass of
acetaminophen
= mol x g/mol
= g
Hence, 109 gm of p-aminophenol gives 151.609 gm of Acetaminophen

→ 1.5 gm of salicylic acid gives ? gm of Acetaminophen
Grams of Acetaminophen obtained = _____X_____
= gm
Practical Yield
Weight of Acetaminophen obtained on drying : _______ gm
Page 31 of 32
Lab Manual
% yield of Acetaminophen
Theoretical Yield
= ________
Melting point
Melting point of Acetaminophen as obtained : ______ °C
Results:
 Theoretical yield of acetaminophen : ______ gm
 Experimental yield of acetaminophen : ______ gm
 % yield of acetaminophen prepared : ______
 Melting point of acetaminophen prepared : ______
- - - -
***
Page 32 of 32

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INDEX

By: - Prof. D. N. Yadav

Determination of Melting Point of the Aspirin Sample

Hence, 138 gm of salicylic acid gives 180gm of Aspirin

Grams of Aspirin obtained = _____X_____

Aim: To prepare P- Acetyl aminophenol.

Chemicals: p-amino phenol, water, acetic anhydride

Moles of p-aminophenol = mass of p-aminophenol taken /molar mass

Moles of acetic anhydride = mass of acetic anhydride taken/molar mass

Hence, Theoretical Yield

Grams of Acetaminophen obtained = _____X_____

Determination of Melting Point of the Anthraquinone Sample

Grams of Anthraquinone obtained = _____X_____

Determination of Melting Point of the Acetanilide Sample

Moles of aniline = mass of aniline / molar mass

Grams of acetic anhydride taken = Volume * Density

Moles of acetic anhydride taken = mass of acetic anhydride/ molar mass

Grams of acetic acid taken = Volume * Density

Finding the Theoretical Yield,

Hence, 102 gm of acetic anhydride gives 135 gm of Acetanilide

Grams of Acetanilide obtained = _____X_____

Aim: To prepare methyl salicylate by esterification of salicylic acid and to determine

Grams of Methanol taken = Volume * Density

Moles of Methanol = mass of Methanol / molar mass

Grams of Salicylic Acid taken = gm

Finding the Theoretical Yield,

Hence, 138 gm of salicylic acid gives 152 gm of Methyl Salicylate

Grams of Methyl Salicylate obtained = _____X_____

% yield of Methyl Salicylate

Aim: To extract sugar from beet.

% Yield of Sugar Obtained = Weight of sugar extracted

Aim: To prepare Nitrobenzene by direct nitration of benzene.

Grams of Nitric Acid taken = Volume * Density

Moles of Nitric Acid = mass of Nitric Acid / molar mass

Grams of Sulfuric Acid taken = Volume * Density

Moles of Sulfuric Acid = mass of Sulfuric Acid / molar mass

Grams of Benzene taken = Volume * Density

Moles of Benzene = mass of Benzene / molar mass

Finding the Theoretical Yield,

Hence, 78 gm of benzene gives 123 gm of Nitrobenzene

Grams of Nitrobenzene obtained = _____X_____

Grams of Nitrobenzene obtained = Volume * Density

Aim: To prepare phenolphthalein form phenol and phatlic anhydride and to

Grams of Phenol taken = Volume * Density

Moles of Phenol = mass of Nitric Acid / molar mass

Grams of Sulfuric Acid taken = Volume * Density

Moles of Sulfuric Acid = mass of Sulfuric Acid / molar mass

Hence, 148 gm of Pthalic anhydride gives 123 gm of Phenolphthalein

Grams of Phenolphthalein obtained = _____X_____

Grams of Phenolphthalein obtained =________ gm

4FeCl36H2O + 3K4(Fe(CN)6)3H2O  Fe4(Fe(CN)6)314H2O +12 KCl

Moles of Potassium Cyanide = mass of Potassium Ferro Cyanide taken /molar

Moles of Ferrous Ammonium Sulfate = mass of Ferrous Ammonium Sulfate taken/molar

Hence, Theoretical Yield

Grams of Prussian Blue obtained = _____X_____

% yield of Prussian Blue

Aim: To prepare Acetaminophen from p-aminophenol, acetic anhydride and to

Determination of Melting Point of the Acetaminophen Sample

Grams of Aspirin obtained = _X_

Grams of Acetaminophen obtained = _X_

Grams of Anthraquinone obtained = _X_

Grams of Acetanilide obtained = _X_

Grams of Methyl Salicylate obtained = _X_

Grams of Nitrobenzene obtained = _X_

Grams of Phenolphthalein obtained = _X_

Grams of Prussian Blue obtained = _X_

Grams of Acetaminophen obtained = _X_